CN108163894B - Ultrahigh-concentration stripping method for transition metal sulfide - Google Patents
Ultrahigh-concentration stripping method for transition metal sulfide Download PDFInfo
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 51
- -1 transition metal sulfide Chemical class 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 58
- 239000002002 slurry Substances 0.000 claims abstract description 36
- 239000002244 precipitate Substances 0.000 claims abstract description 31
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- 238000007865 diluting Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 31
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical group S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 29
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 29
- 239000006185 dispersion Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 10
- ICLYJLBTOGPLMC-KVVVOXFISA-N (z)-octadec-9-enoate;tris(2-hydroxyethyl)azanium Chemical compound OCCN(CCO)CCO.CCCCCCCC\C=C/CCCCCCCC(O)=O ICLYJLBTOGPLMC-KVVVOXFISA-N 0.000 claims description 8
- 239000000344 soap Substances 0.000 claims description 8
- 229940117013 triethanolamine oleate Drugs 0.000 claims description 8
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- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
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- 238000004299 exfoliation Methods 0.000 claims description 4
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 2
- 229960000686 benzalkonium chloride Drugs 0.000 claims description 2
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 claims description 2
- 229940067606 lecithin Drugs 0.000 claims description 2
- 235000010445 lecithin Nutrition 0.000 claims description 2
- 239000000787 lecithin Substances 0.000 claims description 2
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- XEIPQVVAVOUIOP-UHFFFAOYSA-N [Au]=S Chemical compound [Au]=S XEIPQVVAVOUIOP-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
Abstract
The invention provides an ultrahigh concentration method of transition metal sulfide. The method comprises the following specific steps: (1) mixing the transition metal sulfide and the water solution or organic solvent solution of the auxiliary agent, and acting in a ball mill or a sand mill for a period of time to form viscous slurry; (2) diluting the formed thick slurry with a corresponding solvent, stirring for half an hour, standing and layering, wherein the upper layer is the stripped transition metal sulfide suspension and precipitates into a thick-layer transition metal sulfide which is not completely stripped; (3) and (3) after the precipitate in the step (2) is collected, ball milling or sand milling is carried out again for a period of time, so that the stripping yield is further improved. After two treatments, the complete stripping of the transition metal sulfide can be realized. The highest stripping concentration of the invention can reach 1000 mg/mL. The preparation process is safe and controllable, has high efficiency, is easy for industrial amplification, and does not cause pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of materials, and relates to an ultrahigh-concentration stripping method of a transition metal sulfide, in particular to a method for forming viscous slurry after ball milling or sand milling a transition metal sulfide body in an aqueous solution or an organic solution of an auxiliary agent for a period of time; diluting the formed slurry with water or a corresponding solvent, stirring for 30 minutes, standing for layering, wherein the upper layer is the stripped transition metal sulfide dispersion liquid, and the lower layer is precipitated as an incompletely stripped part; and after the lower layer precipitate is collected, the complete stripping of the transition metal sulfide can be realized through secondary sand grinding or ball milling treatment.
Background
Since the discovery of graphene in 2004, two-dimensional materials including transition metal sulfides, transition metal oxides/hydroxides, and boron nitride have attracted extensive attention in both academia and industry due to their excellent combination of properties. Different from zero-band-gap graphene, transition metal sulfide has a band gap, so that the transition metal sulfide is endowed with abundant optical properties, and has wide application prospects in the fields of energy conversion and biology. In addition, the transition metal sulfide also shows excellent properties in the fields of catalysis, lithium batteries, polymer composite materials, super lubrication and the like, and has great research value.
In order to realize the large-scale application of the transition metal sulfide, the development of a simple, efficient, low-cost and low-pollution preparation method is very important. Similar to the preparation method of graphene, the preparation methods of transition metal sulfides can be classified into top-down and bottom-up large-scale. Among them, the liquid phase stripping method using a transition metal sulfide as a bulk material is a top-down method which is considered to have a good industrial prospect. The method generally comprises the steps of dispersing transition metal sulfide in a proper organic solvent or a surfactant aqueous solution, and realizing the stripping of the transition metal sulfide under the action of strong external force such as ultrasound, shearing or ball milling. However, the conventional liquid phase exfoliation method generally has a low yield, and the dispersion concentration of the exfoliated product is low, so that the production cost is high, and it is difficult to scale up the production. Therefore, it is important to develop a method for preparing transition metal sulfides which is low in cost, simple and efficient, and easy to scale up industrially.
Disclosure of Invention
The present invention has been made to overcome the above-mentioned problems, and an object of the present invention is to provide a method for stripping a transition metal sulfide at an ultra-high concentration. The invention adopts a ball milling or sanding action mode, has high stripping concentration and yield close to 100 percent, and is easy for industrial amplification. The transition metal sulfide prepared by the invention can be dispersed in water and other organic solvents, and can be applied to the fields of energy storage, catalysis, composite materials and the like.
In order to achieve the purpose, the invention adopts the technical scheme that: the ultrahigh-concentration stripping method of the transition metal sulfide is characterized by comprising the following specific steps of:
mixing the transition metal sulfide powder with an aqueous solution or an organic solution of an auxiliary agent, and performing action in a ball mill or a sand mill until viscous slurry is formed; wherein the auxiliary agent is selected from any one of triethanolamine oleate soap, dioctyl sodium sulfosuccinate, benzalkonium chloride, lecithin and polysorbate;
diluting the viscous slurry obtained in the step (1) with water or a corresponding organic solvent, stirring, standing and layering, wherein the upper layer is stripped transition metal sulfide dispersion liquid, and the lower layer is precipitate;
and (3) collecting the precipitate obtained in the step (2), and performing secondary action by using a sand mill or a ball mill to obtain the completely stripped transition metal sulfide.
The relevant content in the technical scheme of the preparation method is explained as follows:
1. in the scheme, the transition metal sulfide is molybdenum disulfide or tungsten disulfide, raw materials are directly used without being processed, and the size of the transition metal sulfide body is 500 nm-50 microns.
2. In the scheme, the dosage of the auxiliary agent is 0.1-10 times of the mass of the transition metal sulfide powder.
3. In the scheme, the stripping concentration of the transition metal sulfide obtained in the step (3) is 50-1000 mg/mL.
4. In the above scheme, the organic solvent used in step (1) and step (2) is any one of ethanol, methanol, N dimethylformamide, N-methylpyrrolidone, and ethylene glycol.
5. In the scheme, the rotating speed of the sand mill or the ball mill in the step (1) is 150-1600 rpm, and the time of sand milling or ball milling is 3-24 h.
6. In the scheme, the rotating speed of the sand mill or the ball mill in the step (2) is 150-1600 rpm, and the time of sand milling or ball milling is 3-12 h.
Aiming at the defects in the prior art, the inventor provides the technical scheme of the invention through long-term practice and research, and the transition metal sulfide is taken as a raw material, and is stripped at high concentration and high yield in a ball milling or sanding mode in an auxiliary water solution. The scheme can realize the high-efficiency, low-cost and large-scale preparation of the transition metal sulfide, solves the key problem of large-scale preparation of the transition metal sulfide, and provides an effective way for realizing the practical application of the transition metal sulfide in various fields (such as energy storage materials, composite materials, catalysis and super lubrication). The adjuvant adopted by the invention is a surfactant with larger molecular size, and can effectively inhibit the agglomeration of stripped metal sulfides; the surfactant has higher surface activity and is easier to adsorb on a two-phase interface, and a molecular ordered assembly formed by the surfactant has some special properties and functions which can promote the stripping of the metal oxide under the external acting force; in addition, the surfactant adopted by the invention has certain functionality, and functional products can be further developed according to actual needs.
Compared with the prior art, the invention has the following advantages:
(1) the commercial transition gold sulfide powder can be directly purchased as a raw material, the raw material source is wide, and the cost is low.
(2) The invention can realize the ultra-high concentration stripping of the transition metal sulfide, and the highest stripping concentration can reach 1000 mg/mL.
(3) The method is simple and easy to implement, can realize the complete stripping of the transition metal sulfide, and is easy for industrial amplification.
(4) The transition metal sulfide obtained in the invention can be dispersed in water and organic solvent, and the dispersion concentration can reach more than 20 mg/mL.
In conclusion, complete stripping of transition metal sulfides can be achieved after two treatments. The highest stripping concentration of the invention can reach 1000 mg/mL. The preparation process is safe and controllable, has high efficiency, is easy for industrial amplification, and does not cause pollution to the environment. Compared with the traditional method, the method has low cost, effectively solves the problem of macroscopic preparation of the transition metal sulfide, and lays a foundation for realizing large-scale application of the transition metal sulfide.
Drawings
FIG. 1 is a transmission electron microscope photograph of the molybdenum disulfide obtained in example 1, from which it can be seen that the size of the molybdenum disulfide nanosheet obtained by stripping is between 100 and 200 nm, and the transparent appearance indicates that the obtained molybdenum disulfide is of a few-layer structure;
FIG. 2 is a transmission electron microscope photograph of tungsten disulfide obtained in example 5, from which it can be seen that the size of tungsten disulfide nanosheet obtained by peeling is between 150-200 nm, and the transparent appearance indicates that the obtained tungsten disulfide is of a few-layer structure;
FIG. 3 is an ultraviolet spectrum of the molybdenum disulfide obtained in example 2, from which it can be seen that characteristic peaks appear at 409nm, 489nm, 611nm and 685nm of the ultraviolet spectrum of the molybdenum disulfide dispersion, indicating that molybdenum disulfide is successfully stripped;
FIG. 4 is an ultraviolet spectrum of tungsten disulfide obtained in example 7, from which it can be seen that the ultraviolet spectrum of the tungsten disulfide dispersion has characteristic peaks at 412nm, 461nm, 629nm and 644nm, indicating successful peeling of tungsten disulfide.
Detailed Description
The invention is further described below with reference to the following figures and examples:
example 1
(1) Dissolving 1g triethanolamine oleate soap in 20mL deionized water under stirring, adding the solution and 10g molybdenum disulfide into a ball milling tank after complete dissolution, adding ball milling beads, and carrying out ball milling for 20h under the condition of 300rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide.
(3) The precipitate of (2) was collected and ball milled for 10h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 2
(1) 1g of dioctyl sodium sulfosuccinate is dissolved in 40mL of deionized water under the stirring condition, after complete dissolution, the solution and 10g of molybdenum disulfide are added into a ball milling tank, ball milling beads are added, and ball milling is carried out for 24 hours under the condition of 300rpm, so as to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide.
(3) The precipitate of (2) was collected and ball milled for 12h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 3
(1) 1g of dioctyl sodium sulfosuccinate is dissolved in 40mL of deionized water under the stirring condition, after complete dissolution, the solution and 10g of molybdenum disulfide are added into a ball milling tank, ball milling beads are added, and ball milling is carried out for 24 hours under the condition of 400rpm, so as to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide.
(3) The precipitate of (2) was collected and ball milled for 12h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 4
(1) Dissolving 1g triethanolamine oleate soap in 20mL N-methyl pyrrolidone under stirring, adding the solution and 10g molybdenum disulfide into a ball milling tank after complete dissolution, adding ball milling beads, and carrying out ball milling for 18h at 300rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of N-methylpyrrolidone, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide.
(3) The precipitate of (2) was collected and ball milled for 9h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 5
(1) Dissolving 1g triethanolamine oleate soap in 20mL N, N-dimethylformamide under stirring, adding the solution and 10g molybdenum disulfide into a sanding tank after complete dissolution, adding ball milling beads, and sanding for 24h at 600rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480ml of N-dimethylformamide, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide.
(3) The precipitate from (2) was collected and sanded for 11h, with the other operating conditions being the same as in (1). After secondary sanding, the precipitate in (2) was completely peeled off.
Example 6
(1) Dissolving 1g of sodium dioctyl sulfosuccinate in 20mL of sodium dioctyl sulfosuccinate under stirring, adding the solution and 10g of tungsten disulfide into a ball milling tank after complete dissolution, adding ball milling beads, and carrying out ball milling for 12h under the condition of 400rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of sodium dioctyl sulfosuccinate, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate of (2) was collected and ball milled for 6h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 7
(1) Dissolving 1g triethanolamine oleate soap in 20mL deionized water under stirring, adding the solution and 10g tungsten disulfide into a ball milling tank after complete dissolution, adding ball milling beads, and performing ball milling for 20h under the condition of 300rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate of (2) was collected and ball milled for 10h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 8
(1) 1g of dioctyl sodium sulfosuccinate is dissolved in 40mL of deionized water under the stirring condition, after complete dissolution, the solution and 10g of tungsten disulfide are added into a ball milling tank, ball milling beads are added, and ball milling is carried out for 24 hours under the condition of 300rpm, so as to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate of (2) was collected and ball milled for 12h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 9
(1) 1g of dioctyl sodium sulfosuccinate is dissolved in 40mL of deionized water under the stirring condition, after complete dissolution, the solution and 10g of tungsten disulfide are added into a ball milling tank, ball milling beads are added, and ball milling is carried out for 24 hours under the condition of 400rpm, so as to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate of (2) was collected and ball milled for 12h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 10
(1) Dissolving 1g triethanolamine oleate soap in 20mL N-methyl pyrrolidone under stirring, adding the solution and 10g tungsten disulfide into a ball milling tank after complete dissolution, adding ball milling beads, and carrying out ball milling for 18h at 300rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of N-methylpyrrolidone, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate of (2) was collected and ball milled for 9h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Example 11
(1) Dissolving 1g triethanolamine oleate soap in 20mL N, N-dimethylformamide under stirring, adding the solution and 10g tungsten disulfide into a sanding tank after complete dissolution, adding ball milling beads, and sanding for 24h at 600rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480ml of N-dimethylformamide, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate from (2) was collected and sanded for 11h, with the other operating conditions being the same as in (1). After secondary sanding, the precipitate in (2) was completely peeled off.
Example 12
(1) Dissolving 1g of sodium dioctyl sulfosuccinate in 20mL of sodium dioctyl sulfosuccinate under stirring, adding the solution and 10g of tungsten disulfide into a ball milling tank after complete dissolution, adding ball milling beads, and carrying out ball milling for 12h under the condition of 400rpm to obtain viscous slurry.
(2) The viscous slurry obtained in (1) was diluted with 480mL of sodium dioctyl sulfosuccinate, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped tungsten disulfide dispersion liquid, and the lower layer is incompletely stripped tungsten disulfide.
(3) The precipitate of (2) was collected and ball milled for 6h, with the other operating conditions being the same as in (1). After the secondary ball milling, the precipitate in (2) is completely stripped.
Comparative example 1
(1) Adding 20mL of deionized water and 10g of molybdenum disulfide into a ball milling tank, adding ball milling beads, and carrying out ball milling for 20h at 300rpm to obtain slurry.
(2) The slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide. The results show that only a small amount of molybdenum disulfide peels off.
Comparative example 2
(1) Adding 20mL of N-methylpyrrolidone and 10g of tungsten disulfide into a ball milling tank, adding ball milling beads, and carrying out ball milling for 20h at 300rpm to obtain slurry.
(2) The slurry obtained in (1) was diluted with 480mL of deionized water, stirred for 30 minutes, and then allowed to stand for separation. The upper layer is stripped molybdenum disulfide dispersion liquid, and the lower layer is incompletely stripped molybdenum disulfide. The results show that only a small amount of tungsten disulfide peels off.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. The ultrahigh-concentration stripping method of the transition metal sulfide is characterized by comprising the following specific steps of:
mixing the transition metal sulfide powder with an aqueous solution or an organic solution of an auxiliary agent, and performing action in a ball mill or a sand mill until viscous slurry is formed; wherein the auxiliary agent is selected from any one of triethanolamine oleate soap, dioctyl sodium sulfosuccinate, benzalkonium chloride, lecithin and polysorbate; the dosage of the auxiliary agent is 0.1-10 times of the mass of the transition metal sulfide powder; the rotating speed of the sand mill or the ball mill in the step (1) is 150-1600 rpm, and the sand milling or ball milling time is 3-24 h;
diluting the viscous slurry obtained in the step (1) with water or a corresponding organic solvent, stirring, standing and layering, wherein the upper layer is stripped transition metal sulfide dispersion liquid, and the lower layer is precipitate; the rotating speed of the sand mill or the ball mill in the step (2) is 150-1600 rpm, and the sand milling or ball milling time is 3-12 h;
and (3) collecting the precipitate obtained in the step (2), and performing secondary action by using a sand mill or a ball mill to obtain the completely stripped transition metal sulfide.
2. The ultra-high concentration exfoliation method of transition metal sulfides according to claim 1, characterized in that: the transition metal sulfide is molybdenum disulfide or tungsten disulfide.
3. The ultra-high concentration exfoliation method of transition metal sulfides according to claim 1, characterized in that: the stripping concentration of the transition metal sulfide obtained in the step (3) is 50-1000 mg/mL.
4. The ultra-high concentration exfoliation method of transition metal sulfides according to claim 1, characterized in that: the organic solvent used in the step (1) and the step (2) is any one of ethanol, methanol, N-dimethylformamide, N-methylpyrrolidone and ethylene glycol.
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